Acetic Anhydride → HCID 22556957, compound

Participants

Reaction Steps

Acetic anhydride (1.1 eq, 0.77 ml, in 7 ml of AcOH) was added drop wise to a stirring solution of 3 g of 18 in 34 ml of acetic acid at ambient temperature under N2 over several minutes. HPLC 15 minutes thereafter indicated formation of a hydrophobic product. A catalytic amount of Pd/C (10% w/w) was added to the reaction mixture and teh reaction vessel then was charged with H2 (atm.). The reaction mixture was agitated for about 1.5 h. The agitated reaction mixture was passed through a celite pad (rinsed with ACOH). The filtrate was diluted with ethyl acetate to yield a precipitate. The colid was isolated and dried in vacuo to yield 2.05 g of the crude amdidine.

Provenance & Evidence